CN104356591A - Toughened enhanced phenolic foam insulation material and preparation method thereof - Google Patents
Toughened enhanced phenolic foam insulation material and preparation method thereof Download PDFInfo
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- CN104356591A CN104356591A CN201410617939.2A CN201410617939A CN104356591A CN 104356591 A CN104356591 A CN 104356591A CN 201410617939 A CN201410617939 A CN 201410617939A CN 104356591 A CN104356591 A CN 104356591A
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Abstract
The invention relates to a toughened enhanced phenolic foam insulation material. The material is characterized by mainly comprising the following raw materials: 100 parts of phenolic resin, 2-10 parts of phenolic resin fluidity improver, 5-15 parts of emulsifying agent, 4-8 parts of foaming agent, 1-10 parts of toughening-enhancing agent, and 6-55 parts of reactivity acid curing agent. The reactivity acid curing agent in high additive amount is adopted so that the cost is lowered, and the system residual acid is small and the corrosivity is small. The glass fiber powder and diatomite are used as the toughening-enhancing agent so that the foam flame retardation is improved, and the production cost is lowered.
Description
Technical field
The present invention relates to a kind of preparation method of toughen and intensify type phenolic aldehyde foam thermal insulation material, belong to the category of synthesized polymer material.Toughen and intensify type phenolic aldehyde foam thermal insulation material prepared by the present invention can be used for the industry heat-insulation and heat-preservations such as building exterior wall heat preserving, ventilator trunk, petrochemical pipe, electrical equipment, instrument.
Background technology
The porous plastics such as polystyrene, polyethylene, urethane, because of features such as thermal conductivity is low, lightweight, easy constructions, are used widely in fields such as external wall heat-insulation and heat-preservation, ventilator trunk, petrochemical pipe insulations.But now widely used several porous plastics also exists the shortcomings such as easy firing, the amount of being fuming is large, toxicity is high, heat resisting temperature is low as urethane, polystyrene etc., its application in external wall, marine piping, the insulation of high temperature petrochemical pipe etc. is very limited.And phenolic foamed plastics have fire resistance good, do not burn, the advantage such as the amount of being fuming is little, fire penetration resistance is good, a kind of fire prevention of excellent performance, heat insulation, sound insulation, lightweight, energy-saving material, thermal conductivity only has 0. 018 0. 042ff/mk, heat-insulating property is better than polystyrene, urethane, polyethylene etc., the lagging material that heat insulation effect is more traditional than mineral wool, jelutong bukit, perlite, glass wool etc. is high more than 1 times, have again simultaneously the foams such as polystyrene, urethane, polyethylene far away from flame retardant property.Exist in current phenolic foamed plastics production process: (1) system viscosity is large, material transfer difficulty; (2) lower boiling alkane and hydrochloric ether is used to make whipping agent, to environmental danger; (3) foam bubble hole uneven, affect heat conductivility; (4) foams toughness, intensity are low, fall slag rate high; (5) resin originating party amount is little, foam cost height more obvious than polystyrene foam, affects its spread and uses.
Summary of the invention
The present invention is directed to the preparation method that the problems referred to above disclose a kind of phenol formaldehyde foam, the present invention adopts ethylene bis stearamide (EBS) and Tegin 55G as resol fluidity improver in phenol formaldehyde foam preparation technology, reduces the viscosity of phenolic foam system; Adopt methylal Substitute For Partial lower boiling alkane and hydrochloric ether as environmentally friendly whipping agent; Polyoxyethylene grafting methyl water-based silicone oil or block type aqueous dimethylformamide silicone oil is adopted to be foam emulsion stablizer; Adopt glass fiber powder and diatomite as toughness reinforcing, strengthen and fire retardant; Adopt sulfonation polyoxyethylene nonylphenol ether, sulfonation cardanol, sulfonated castor oil and Neville acid to be reactive acid solidifying agent, higher addition can be adopted, to reduce costs and system residual acid is little, corrodibility is little; The phenol formaldehyde foam prepared by present method has uniform foam cell, exquisiteness, intensity are high, good toughness, falls the features such as slag rate is low, reactive acid solidifying agent addition content is large, cost is low.Solve that phenol formaldehyde foam easily falls slag, matter is crisp, intensity is low, poor toughness, high in cost of production shortcoming, maintain again the traditional advantages such as low, the low cigarette of phenol formaldehyde foam thermal conductivity, superior flame retardant property.
Technical solution of the present invention is: a kind of toughen and intensify type phenolic aldehyde foam thermal insulation material, is prepared from primarily of following raw material:
Resol: 100 parts
Resol fluidity improver: 2-10 part
Whipping agent: 4-8 part
Emulsifying agent: 5-15 part
Toughness reinforcing, toughener: 1-10 part
Reactive acid solidifying agent: 6-55 part.
Foregoing toughen and intensify type phenolic aldehyde foam thermal insulation material, preferably, is prepared from primarily of following raw material:
Resol: 100 parts
Resol fluidity improver: 4-8 part
Whipping agent: 5-7 part;
Emulsifying agent: 7-12 part
Toughness reinforcing, toughener: 3-8 part
Reactive acid solidifying agent: 12-45 part.
Foregoing toughen and intensify type phenolic aldehyde foam thermal insulation material, preferably, is prepared from primarily of following raw material:
Resol: 100 parts
Resol fluidity improver: 6 parts
Whipping agent: 6 parts;
Emulsifying agent: 10 parts
Toughness reinforcing, toughener: 6 parts
Reactive acid solidifying agent: 20 parts.
Foregoing toughen and intensify type phenolic aldehyde foam thermal insulation material, preferably, described resol is common resole or Aromatic Polyester Polyols modified phenolic resins.
Foregoing toughen and intensify type phenolic aldehyde foam thermal insulation material, preferably, described resol fluidity improver is one in EBS, Tegin 55G or two kinds and above mixture.
Foregoing toughen and intensify type phenolic aldehyde foam thermal insulation material, preferably, described reactive acid solidifying agent is one or two kinds and the above mixture of sulfonation polyoxyethylene nonylphenol ether, sulfonation cardanol, sulfonated castor oil and Neville acid.
Foregoing toughen and intensify type phenolic aldehyde foam thermal insulation material, preferably, described toughness reinforcing, toughener is for glass fiber powder and diatomite press the mixture of 80:20-60:40 mass ratio.Wherein glass fiber powder specification: particle diameter 400-800 order, water ratio <0.5%, density 2.20-2.35g/cm
3; Diatomite specification is: moisture content≤2%, SiO
2content>=65.0% Fe
2o
3content≤5.1%, density 1.90-2.30g/cm
3, specific surface area 40-65m
2/ g.
Foregoing toughen and intensify type phenolic aldehyde foam thermal insulation material, preferably, first resol and emulsifying agent, resol fluidity improver, toughness reinforcing, toughener high-speed stirring are mixed, finally add reactive acid solidifying agent to mix, be transferred in the mould of preheating, put into 60-70 ° of C baking oven, be incubated foaming in 6-12 hour, slaking 24 hours, the demoulding, obtain product.
The present invention relates to a kind of preparation method of modified toughened enhancement type phenolic aldehyde foam thermal insulation material.The present invention adopts ethylene bis stearamide (EBS) and Tegin 55G as resol fluidity improver in phenol formaldehyde foam preparation technology, reduces the viscosity of phenolic foam system; Adopt methylal Substitute For Partial lower boiling alkane and hydrochloric ether as environmentally friendly whipping agent; Polyoxyethylene grafting or block type aqueous dimethylformamide silicone oil is adopted to be foam emulsion stablizer; Adopt glass fiber powder and diatomaceous mixture as toughness reinforcing, strengthen and fire retardant; Sulfonation polyoxyethylene nonylphenol ether, sulfonation cardanol, sulfonated castor oil and Neville acid is adopted to be reactive acid solidifying agent.The phenol formaldehyde foam prepared by present method has uniform foam cell, exquisiteness, intensity are high, good toughness, falls the features such as slag rate is low, reactive acid solidifying agent addition content is large, cost is low.Solve that phenol formaldehyde foam easily falls slag, matter is crisp, intensity is low, poor toughness, high in cost of production shortcoming, maintain again the traditional advantages such as low, the low cigarette of phenol formaldehyde foam thermal conductivity, superior flame retardant property.
Advantage of the present invention is also embodied in:
1, adopt ethylene bis stearamide (EBS), Tegin 55G, as internal lubricant, improves resol mobility, reduces its bulk viscosity;
2, adopt reactable acid to make solidifying agent, not only play catalysis, solidification, also become a resin body part, addition content is many simultaneously, but residual acid is few, and system acidity is little, little to materials for wall corrodibility; And cost is low, originating party amount is large;
3. adopt glass fiber powder and diatomaceous mixture to be toughness reinforcing, toughener and foam flame retardant properties can be improved.
Embodiment
Below by embodiment, the present invention is described in further detail.
The raw materials used Aromatic Polyester Polyols modified phenolic resins of the present invention, sulfonation polyoxyethylene nonylphenol ether and sulfonation cardanol are self-control; Other raw materials all can be bought from market.
Preparation method is as follows for Aromatic Polyester Polyols modified phenolic resins:
First prepare Aromatic Polyester Polyols
:ethylene glycol, glycol ether, Triethylene glycol, dipropylene glycol, glycerine are added reactor, warming while stirring, then under agitation adds terephthalic acid, m-phthalic acid, phthalic anhydride, then titanic acid ester is added, first control at low temperatures, reaction certain hour, then raised temperature, and held for some time, cooling vacuumizes, and maintain certain hour, cooling discharge obtains product Aromatic Polyester Polyols
.
Prepare toughening modifying resol
:reactor is added after first being dissolved by phenol, add formaldehyde solution, basic catalyst stage by stage again, regulate pH=9, add triphenylphosphate or triphenyl phosphite or triphenyl borate and make resol prepolymer at a certain temperature, add the Aromatic Polyester Polyols of above-mentioned preparation again, regulate reaction solution pH=5 with formic acid, continue to react 1h at 85 DEG C-90 DEG C, add basic solution and regulate pH=7.5, make mixture be cooled to rapidly 75 DEG C with cooling bath; Decompression dehydration 1-1.5h at 75 DEG C, viscosity controller, at 20-30mPas, obtains toughening modifying resol
.
Preparation method is as follows for sulfonation polyoxyethylene nonylphenol ether:
In reaction flask, add 100 parts of polyoxyethylene nonylphenol ethers, 20 parts of Diethylene Glycols, start stirring, temperature control 20-30 DEG C under agitation slowly (in 60-90 minute) drip 60 parts of vitriol oils; Slowly heat up after adding acid 80-85 DEG C, reacts 3 hours, be cooled to 40 DEG C, then add 10 parts of Diethylene Glycols, discharging.
Preparation method is as follows for sulfonation cardanol:
In reaction flask, add 100 parts of cardanols, temperature control 20-30 DEG C, under agitation slowly (in 60 minutes) drip 50 parts of vitriol oils, slowly heat up 85 DEG C after adding acid, react 4 hours, continue reaction 3 hours after adding acid, be cooled to 40 DEG C, add 10 parts of Diethylene Glycols again, discharging.
Normal practice of the present invention: a kind of toughen and intensify type phenolic aldehyde foam thermal insulation material, is prepared from primarily of following raw material:
Resol: 100 parts
Resol fluidity improver: 2-10 part
Whipping agent: 4-8 part
Emulsifying agent: 5-15 part
Toughness reinforcing, toughener: 1-10 part
Reactive acid solidifying agent: 6-55 part.
The preparation method of described toughen and intensify type phenolic aldehyde foam thermal insulation material, first resol and emulsifying agent, resol fluidity improver, toughness reinforcing, toughener high-speed stirring are mixed, finally add reactive acid solidifying agent to mix, be transferred in the mould of preheating, put into 60-70 ° of C baking oven, be incubated foaming in 6-12 hour, slaking 24 hours, the demoulding, obtain product.
Described resol is common resole or Aromatic Polyester Polyols modified phenolic resins.Described resol fluidity improver is one in ethylene bis stearamide (EBS), Tegin 55G or two kinds and above mixture.Described reactive acid solidifying agent is one or two kinds and the above mixture of sulfonation polyoxyethylene nonylphenol ether, sulfonation cardanol, sulfonated castor oil and Neville acid; Described toughness reinforcing, toughener is glass fiber powder and diatomaceous mixture.
Embodiment 1
Successively resol and emulsifying agent, suds-stabilizing agent, Resin Flow improving agent, toughness reinforcing, toughener high-speed stirring are mixed by following formula, and then it is even to add composite foamable agent powerful mixing, finally add reactive acid solidifying agent to mix, be transferred in the mould of preheating, put into 65 ° of C baking ovens, be incubated foaming in 8 hours, slaking 24 hours, the demoulding, obtain phenolic foam products 1.
Resol: 100 parts
Resol fluidity improver: 10 parts
Whipping agent: 6 parts
Emulsifying agent: 15 parts
Toughness reinforcing, toughener: 10 parts
Reactive acid solidifying agent: 55 parts.
Embodiment 2
Successively resol and emulsifying agent, suds-stabilizing agent, Resin Flow improving agent, toughness reinforcing, toughener high-speed stirring are mixed by following formula, and then it is even to add composite foamable agent powerful mixing, finally add reactive acid solidifying agent to mix, be transferred in the mould of preheating, put into 70 ° of C baking ovens, be incubated foaming in 8 hours, slaking 24 hours, the demoulding, obtain phenolic foam products 2.
Aromatic Polyester Polyols modified phenolic resins: 100 parts
Resol fluidity improver: 5 parts
Whipping agent: 6 parts
Emulsifying agent: 8 parts
Toughness reinforcing, toughener: 1.5 parts
Reactive acid solidifying agent: 45 parts.
Embodiment 3
Successively resol and emulsifying agent, suds-stabilizing agent, Resin Flow improving agent, toughness reinforcing, toughener high-speed stirring are mixed by following formula, and then it is even to add composite foamable agent powerful mixing, finally add reactive acid solidifying agent to mix, be transferred in the mould of preheating, put into 70 ° of C baking ovens, be incubated foaming in 6 hours, slaking 24 hours, the demoulding, obtain phenolic foam products 3.
Aromatic Polyester Polyols modified phenolic resins: 100 parts
Resol fluidity improver: 4 parts
Whipping agent: 6 parts
Emulsifying agent: 7 parts
Toughness reinforcing, toughener: 1.5 parts
Reactive acid solidifying agent: 35 parts.
Embodiment 4
Successively resol and emulsifying agent, suds-stabilizing agent, Resin Flow improving agent, toughness reinforcing, toughener high-speed stirring are mixed by following formula, and then it is even to add composite foamable agent powerful mixing, finally add reactive acid solidifying agent to mix, be transferred in the mould of preheating, put into 70 ° of C baking ovens, be incubated foaming in 7 hours, slaking 24 hours, the demoulding, obtain phenolic foam products 4.
Resol: 100 parts
Resol fluidity improver: 6 parts
Whipping agent: 6 parts
Emulsifying agent: 10 parts
Toughness reinforcing, toughener: 6 parts
Reactive acid solidifying agent: 20 parts.
Embodiment 5
Successively resol and emulsifying agent, suds-stabilizing agent, Resin Flow improving agent, toughness reinforcing, toughener high-speed stirring are mixed by following formula, and then it is even to add composite foamable agent powerful mixing, finally add reactive acid solidifying agent to mix, be transferred in the mould of preheating, put into 70 ° of C baking ovens, be incubated foaming in 7 hours, slaking 24 hours, the demoulding, obtain phenolic foam products 5.
Resol: 100 parts
Resol fluidity improver: 6 parts
Whipping agent: 6 parts
Emulsifying agent: 10 parts
Reactive acid solidifying agent: 25 parts.
Gained phenol formaldehyde foam salient features is as following table:
Can find out from upper table experimental result: it is low that phenol formaldehyde foam prepared by toughness reinforcing, the toughener that add glass fiber powder and diatomite composition falls slag rate, and compressive strength is high, and good toughness, thermal conductivity are little, good heat insulating.
Claims (8)
1. a toughen and intensify type phenolic aldehyde foam thermal insulation material, is characterized in that, is prepared from primarily of following raw material:
Resol: 100 parts
Resol fluidity improver: 2-10 part
Whipping agent: 4-8 part
Emulsifying agent: 5-15 part
Toughness reinforcing, toughener: 1-10 part
Reactive acid solidifying agent: 6-55 part.
2. toughen and intensify type phenolic aldehyde foam thermal insulation material according to claim 1, is characterized in that, be prepared from primarily of following raw material:
Resol: 100 parts
Resol fluidity improver: 4-8 part
Whipping agent: 5-7 part;
Emulsifying agent: 7-12 part
Toughness reinforcing, toughener: 3-8 part
Reactive acid solidifying agent: 12-45 part.
3. toughen and intensify type phenolic aldehyde foam thermal insulation material according to claim 1, is characterized in that, be prepared from primarily of following raw material:
Resol: 100 parts
Resol fluidity improver: 6 parts
Whipping agent: 6 parts;
Emulsifying agent: 10 parts
Toughness reinforcing, toughener: 6 parts
Reactive acid solidifying agent: 20 parts.
4., according to the arbitrary described toughen and intensify type phenolic aldehyde foam thermal insulation material of claim 1-3, it is characterized in that, described resol is common resole or Aromatic Polyester Polyols modified phenolic resins.
5. according to the arbitrary described toughen and intensify type phenolic aldehyde foam thermal insulation material of claim 1-3, it is characterized in that, described resol fluidity improver is one in ethylene bis stearic acid amide, Tegin 55G or two kinds and above mixture.
6. according to the arbitrary described toughen and intensify type phenolic aldehyde foam thermal insulation material of claim 1-3, it is characterized in that, described reactive acid solidifying agent is one or two kinds and the above mixture of sulfonation nonylphenol polyoxyethylenes ether, sulfonation cardanol, sulfonated castor oil and Neville acid.
7. according to the arbitrary described toughen and intensify type phenolic aldehyde foam thermal insulation material of claim 1-3, it is characterized in that, described toughness reinforcing, toughener is glass fiber powder and diatomite, and by the mixture of 80:20-60:40 mass ratio, (wherein glass fiber powder specification is: particle diameter 400-800 order, water ratio <0.5%, density 2.20-2.35g/cm
3; Diatomite specification is: moisture content≤2%, SiO
2content>=65.0% Fe
2o
3content≤5.1%, density 1.90-2.30g/cm
3, specific surface area 40-65m
2/ g).
8. according to the preparation method of the arbitrary described toughen and intensify type phenolic aldehyde foam thermal insulation material of claim 1-3, it is characterized in that, first resol and emulsifying agent, resol fluidity improver, toughness reinforcing, toughener high-speed stirring are mixed, finally add reactive acid solidifying agent to mix, be transferred in the mould of preheating, put into 60-70 ° of C baking oven, be incubated foaming in 6-12 hour, slaking 24 hours, the demoulding, obtain product.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104804372A (en) * | 2015-04-17 | 2015-07-29 | 广西藤县通轩立信化学有限公司 | Foaming phenolic resin composition |
| CN106243613A (en) * | 2016-08-01 | 2016-12-21 | 合肥广能新材料科技有限公司 | Phenol formaldehyde foam thermal insulating composite panel and preparation method thereof |
| CN106433015A (en) * | 2016-09-18 | 2017-02-22 | 安徽嘉伟新材料科技有限责任公司 | Hair-reinforced phenolic foam heat-preservation sectional material and preparing method |
| CN106867193A (en) * | 2017-02-22 | 2017-06-20 | 广西芮芽科技有限公司 | Improve the preparation method of phenolic foam material heat-insulating property |
| CN106883550A (en) * | 2017-02-22 | 2017-06-23 | 广西芮芽科技有限公司 | The preparation method of phenolic foam material |
| CN106928645A (en) * | 2017-02-22 | 2017-07-07 | 广西芮芽科技有限公司 | The preparation method of the phenolic foam material with heat insulating ability high |
| CN107325479A (en) * | 2017-07-18 | 2017-11-07 | 合肥广能新材料科技有限公司 | Plasticizing phenol formaldehyde warming plate and preparation method thereof |
| CN107446305A (en) * | 2017-07-18 | 2017-12-08 | 合肥广能新材料科技有限公司 | Phenolic resin warming plate and preparation method thereof |
| CN108102291A (en) * | 2017-12-12 | 2018-06-01 | 常州琨瑶纺织品有限公司 | A kind of light flame-retardant phenolic foam material and preparation method thereof |
| CN109651757A (en) * | 2019-01-02 | 2019-04-19 | 广东明日环保净化有限公司 | A kind of preparation method of high-performance modified phenolic resin cold-storage insulation board |
| CN115612245A (en) * | 2022-10-14 | 2023-01-17 | 山东北理华海复合材料有限公司 | Phenolic resin thermal insulation material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103788570A (en) * | 2012-10-31 | 2014-05-14 | 合肥杰事杰新材料股份有限公司 | Modified phenolic foam and preparation method thereof |
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2014
- 2014-11-06 CN CN201410617939.2A patent/CN104356591B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103788570A (en) * | 2012-10-31 | 2014-05-14 | 合肥杰事杰新材料股份有限公司 | Modified phenolic foam and preparation method thereof |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104804372A (en) * | 2015-04-17 | 2015-07-29 | 广西藤县通轩立信化学有限公司 | Foaming phenolic resin composition |
| CN106243613A (en) * | 2016-08-01 | 2016-12-21 | 合肥广能新材料科技有限公司 | Phenol formaldehyde foam thermal insulating composite panel and preparation method thereof |
| CN106433015A (en) * | 2016-09-18 | 2017-02-22 | 安徽嘉伟新材料科技有限责任公司 | Hair-reinforced phenolic foam heat-preservation sectional material and preparing method |
| CN106867193A (en) * | 2017-02-22 | 2017-06-20 | 广西芮芽科技有限公司 | Improve the preparation method of phenolic foam material heat-insulating property |
| CN106883550A (en) * | 2017-02-22 | 2017-06-23 | 广西芮芽科技有限公司 | The preparation method of phenolic foam material |
| CN106928645A (en) * | 2017-02-22 | 2017-07-07 | 广西芮芽科技有限公司 | The preparation method of the phenolic foam material with heat insulating ability high |
| CN107325479A (en) * | 2017-07-18 | 2017-11-07 | 合肥广能新材料科技有限公司 | Plasticizing phenol formaldehyde warming plate and preparation method thereof |
| CN107446305A (en) * | 2017-07-18 | 2017-12-08 | 合肥广能新材料科技有限公司 | Phenolic resin warming plate and preparation method thereof |
| CN108102291A (en) * | 2017-12-12 | 2018-06-01 | 常州琨瑶纺织品有限公司 | A kind of light flame-retardant phenolic foam material and preparation method thereof |
| CN109651757A (en) * | 2019-01-02 | 2019-04-19 | 广东明日环保净化有限公司 | A kind of preparation method of high-performance modified phenolic resin cold-storage insulation board |
| CN115612245A (en) * | 2022-10-14 | 2023-01-17 | 山东北理华海复合材料有限公司 | Phenolic resin thermal insulation material and preparation method thereof |
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